CN108164132A - A kind of preparation method for mixing yttrium jaundice green light glass - Google Patents
A kind of preparation method for mixing yttrium jaundice green light glass Download PDFInfo
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- CN108164132A CN108164132A CN201711432649.0A CN201711432649A CN108164132A CN 108164132 A CN108164132 A CN 108164132A CN 201711432649 A CN201711432649 A CN 201711432649A CN 108164132 A CN108164132 A CN 108164132A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of preparation method for mixing yttrium jaundice green light glass, first, by Tb2O3, B2O3, Ga2O3, Y2O3, SiO2, GeO2, Sb2O3, SnO2, ZrO2It mixes to the uniformity to be more than after 98% and forms batch；Then, batch is melted into obtain glass metal, glass metal is poured into graphite jig at 250~380 DEG C, be put into after sizing in 710 DEG C of stove keep the temperature 3h after be cooled to room temperature both must mix yttrium turn to be yellow green light glass.The jaundice green light glass luminous intensity of technique preparation is high, brightness is high, glass melting temperature is low, glass forming ability is good, preparation process is simple, thermal stability and chemical stabilization are good.According to the jaundice green light glass product that preparation method of the present invention obtains since with glass inherent transparency, high density, it is easy to prepare, simple process and low cost, suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method for mixing yttrium glass, more particularly to a kind of preparation side for mixing yttrium jaundice green light glass
Method.
Background technology
Luminescence generated by light refers to that object relies on external light source and is irradiated, and so as to obtain energy, generation excitation causes luminous
Phenomenon.After certain substance is excited, substance will be in excitation state, and the energy of excitation state can be discharged by the form of light or heat
Out.If the energy of this part is to be located at visible, ultraviolet or near-infrared electromagnetic radiation, this process is referred to as to shine
Journey.The substance that can be shone after excitation is just called luminescent material.Luminescent material type is various, and principle of luminosity is different, shines
Characteristic is also each has something to recommend him.Luminescent material mainly has embedded photoluminescent material, cathode-ray luminescence material, electroluminescent material, radiation
Luminescent material, light release the types such as luminescent material and thermoluminescence material, and wherein embedded photoluminescent material has a extensive future, each
Field application prospect is huge.It is wherein especially especially noticeable with rare earth luminescent material.
Rare earth is because of its special electron structure, and the spectral quality for having general element incomparable, rare earth luminous
Almost cover the scope of entire solid luminescence.Rare earth element electron energy level enriches, and lifetime of excited state is long.Rare earth luminescent material light
Absorbability is strong, and high conversion efficiency, photoluminescent band is narrow, and excitation purity is high, and bright in luster, light absorpting ability is strong, high conversion efficiency, and object
Reason and stable chemical performance are widely used in illuminating, show, image, the detection of medical radioactive image, radiation field and record etc.
Field forms very big industrial production and consumption market scale.
White light LEDs have the tendency that gradually replacing the traditional lightings means such as incandescent lamp and fluorescent lamp in recent years.Mainly due to
White light LEDs are energy-efficient, long lifespan and environmental protection.The mainstream for realizing white light at present is combination and the core that blue chip adds fluorophor
Piece UV chips add the combination of fluorophor.But only blue chip adds green-yellow light fluorophor YAG：Ce white lights, which disclosure satisfy that, generally will
It asks, is achieved commercialization.But the pattern colour rendering index is relatively low, is used in certain special occasions limited.
At present, white light LEDs yellowish green fluorescent powder mainly has silicate, nitride and molybdate fluorescent powder.Patent
CN101292009B discloses a kind of silicate systems A2SiO4：Eu2+D, A are at least one selected from Sr, Ca, Ba, Zn, Cd；D is
At least one dopant selected from F, Cl, Br, I, P, S, N.The fluorescent powder can be excited effectively between 280~490nm, transmitting
Wavelength is between 460~590nm.But the luminous efficiency of the fluorescent powder prepared by the patent is relatively low, stability is poor, Wu Faman
The demand of sufficient practical application；Eu2+The nitride and nitrogen oxides of activation are also by very big concern.Patent CN102533260A is disclosed
A kind of nitrogen oxides A1-xSiyOzN2/3+4/3y-2/3z：The preparation method of xEu (A=Ca, Sr) fluorophor, the sample emission wavelength
Between 530~45nm, but the synthesis of such fluorescent powder needs high temperature (1600~1800 DEG C), high pressure, and synthesis condition is more severe
It carves, it is very big to the loss of electric energy；(Zhang Weijie, Feng Wenlin, Cheng Xue antelope wait the novel yellowish green fluorescent powders of to Zhang Weijie et al.
BaMoO4:Pr3+Preparation and photoluminescent property study [J] Acta Opticas, 2014,34 (9):201-204.) high using tradition
Warm solid phase method has developed yellowish green fluorescent powder Ba1-xMoO4：xPr3+, this fluorescent powder can have by the blue light of 430~500nm
Effect excitation, emits stronger green-yellow light.But these are irregular using fluorescent powder grain pattern prepared by high temperature solid-state method, granularity
The defects of being distributed extensively, being a very big for as LED fluorescent powder.It will appear mixed powder problem in package application, without glimmering
There are thermal stability difference between light powder, reabsorb and the problems such as light-output.And rare earth ion doped light conversion glass preparation
It is simple for process；It is of low cost；Chemical stability is good；Good thermal stability；Optical quality is high；Processing is closed with LED junction simply, this
A little advantages cause light conversion glass to be known as the potential approach that LED adjusts optical color parameter.
Invention content
The purpose of the present invention is to provide one kind is colourless, transparent, luminous intensity is high, brightness is high, coloration is pure, glass melting temperature
The preparation side for mixing yttrium jaundice green light glass low, glass forming ability is excellent, preparation process is simple, thermal stability and chemical stabilization are excellent
Method.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
1) first, by molar fraction by the Tb of 18~22mol%2O3, the B of 22~26mol%2O3, 11~15mol%'s
Ga2O3, the Y of 2~6mol%2O3, the GeO of 13~17mol%2, the SiO of 20~24mol%2, the Sb of 0~1mol%2O3, 0.3~
The SnO of 1mol%2, the ZrO of 0.3~1mol%2It mixes to being formed uniformly batch；
2) secondly, batch addition has been warming up in 1450~1500 DEG C of platinum crucible, has kept the temperature 30 minutes；
3) furnace temperature then, is cooled to 1380 DEG C by 30 minutes, and keeps the temperature 30min；
4) finally, the glass metal of melting is poured into 250~380 DEG C of graphite jig, 710 DEG C of stove is put into after sizing
In, after keeping the temperature 3h, room temperature is cooled to 1 DEG C/min of rate of temperature fall and mixes yttrium jaundice green light glass up to transparent.
The B2O3It is introduced by analytically pure boric anhydride, GeO2It is introduced by analytically pure germanium dioxide, Tb2O3、Ga2O3、
Y2O3、Sb2O3, SnO2, ZrO2Respectively by analytically pure terbium peroxide, gallium oxide, yttrium oxide, antimony oxide, tin oxide, oxygen
Change zirconium to introduce.
The SiO2Using the quartz sand of 60 mesh, wherein, the content of di-iron trioxide is less than 100ppm in quartz sand.
The step 1) mix to the uniformity be more than 98% after form batch.
The present invention is by high-temperature fusion technique, and without atmosphere protection, fusing in air is prepared for mixing yttrium jaundice green light glass
Glass.The rare earth luminous intensity of jaundice green light glass of technique preparation is high, brightness is high, coloration is pure, glass melting temperature is low, glass forming ability is excellent
Good, preparation process is simple, thermal stability and chemical stabilization are excellent.
Jaundice green light glass product colour stable, the colour rendering index obtained according to preparation method of the present invention is high, color rendition
Property is good；In addition, easy, simple process and low cost is prepared according to the jaundice green light glass product that preparation method of the present invention obtains, it is suitable
In industrialized production.
Description of the drawings
Fig. 1 is that water white transparency prepared by embodiment 1 can turn to be yellow the luminescent spectrum figure of green light glass, and wherein abscissa is transmitting
Optical wavelength, ordinate are emitted luminescence intensity.
Fig. 2 is that water white transparency prepared by embodiment 1 can turn to be yellow the reality under the burst of ultraviolel of 365nm wavelength of green light glass
Object luminous photo.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
B in following embodiment2O3It is introduced by analytically pure boric anhydride, GeO2It is introduced by analytically pure germanium dioxide, SiO2By 60
Purpose quartz sand introduces, wherein, the content of di-iron trioxide is less than 100ppm, Tb in quartz sand2O3、Ga2O3、Y2O3、Sb2O3,
SnO2, ZrO2Respectively by analytically pure terbium peroxide, gallium oxide, yttrium oxide, antimony oxide, tin oxide, zirconium oxide introducing.
Embodiment 1：
1) first, by molar fraction by the Tb of 18mol%2O3, the B of 24mol%2O3, the Ga of 15mol%2O3, 5.2mol%
Y2O3, the GeO of 15mol%2, the SiO of 22mol%2, the SnO of 0.3mol%2, the ZrO of 0.5mol%2It mixes big to the uniformity
Batch is formed after 98%；
2) then, batch addition has been warming up in 1450 DEG C of platinum crucible；Heat preservation 30 minutes；
3) furnace temperature then, is cooled to 1380 DEG C by 30 minutes, and keeps the temperature 30min；
4) finally, the glass metal of melting is poured into 250 DEG C of graphite jig, is put into after sizing in 710 DEG C of stove, kept the temperature
After 3h, with 1 DEG C/min of rate of temperature fall, room temperature is cooled to up to the transparent green light glass that turns to be yellow.
Attached drawing 1 is that the prepared water white transparency green light glass that can turn to be yellow in excitation wavelength is the photoluminescence spectra under 374nm,
Wherein abscissa is wavelength of transmitted light, and ordinate is relative intensity.As seen from Figure 1, it is prepared to mix yttrium jaundice green light glass
Glass, most strong wavelength of transmitted light is 544.2nm, and emitted luminescence intensity is very weak at 490.8nm, 590.4nm, 620.4nm.
Attached drawing 2 is that prepared water white transparency mixes material object of the yttrium jaundice green light glass under the burst of ultraviolel in 365nm wavelength
Luminous photo.As seen from Figure 2, bright yellow green is presented, and sample is transparent in prepared yttrium jaundice green light glass of mixing.
Embodiment 2：
1) first, by molar fraction by the Tb of 21.85mol%2O3, the B of 24mol%2O3, the Ga of 13mol%2O3,
The Y of 2mol%2O3, the GeO of 17mol%2, the SiO of 20mol%2, the Sb of 0.5mol%2O3, the SnO of 1mol%2, 0.65mol%
ZrO2It mixes to the uniformity to be more than after 98% and forms batch；
2) then, batch addition has been warming up in 1460 DEG C of platinum crucible；Heat preservation 30 minutes；
3) furnace temperature then, is cooled to 1380 DEG C by 30 minutes, and keeps the temperature 30min；
4) finally, the glass metal of melting is poured into 315 DEG C of graphite jig, is put into after sizing in 710 DEG C of stove, kept the temperature
After 3h, with 1 DEG C/min of rate of temperature fall, room temperature is cooled to up to the transparent green light glass that turns to be yellow.
Embodiment 3：
1) first, by molar fraction by the Tb of 20mol%2O3, the B of 22mol%2O3, the Ga of 11mol%2O3, 6mol%'s
Y2O3, the GeO of 14.9mol%2, the SiO of 24mol%2, the Sb of 0.6mol%2O3, the SnO of 0.5mol%2, the ZrO of 1mol%2It is mixed
Batch is formed after the uniformity is bonded to more than 98%；
2) then, batch addition has been warming up in 1475 DEG C of platinum crucible；Heat preservation 30 minutes；
3) furnace temperature then, is cooled to 1380 DEG C by 30 minutes, and keeps the temperature 30min；
4) finally, the glass metal of melting is poured into 350 DEG C of graphite jig, is put into after sizing in 710 DEG C of stove, kept the temperature
After 3h, with 1 DEG C/min of rate of temperature fall, room temperature is cooled to up to the transparent green light glass that turns to be yellow.
Embodiment 4：
1) first, by molar fraction by the Tb of 22mol%2O3, the B of 26mol%2O3, the Ga of 12mol%2O3, 4mol%'s
Y2O3, the GeO of 13mol%2, the SiO of 21.05mol%2, the Sb of 1mol%2O3, the SnO of 0.65mol%2, the ZrO of 0.3mol%2
It mixes to the uniformity to be more than after 98% and forms batch；
2) then, batch addition has been warming up in 1500 DEG C of platinum crucible；Heat preservation 30 minutes；
3) furnace temperature then, is cooled to 1380 DEG C by 30 minutes, and keeps the temperature 30min；
4) finally, the glass metal of melting is poured into 380 DEG C of graphite jig, is put into after sizing in 710 DEG C of stove, kept the temperature
After 3h, with 1 DEG C/min of rate of temperature fall, room temperature is cooled to up to the transparent green light glass that turns to be yellow.
The present invention is by high-temperature fusion technique, and without atmosphere protection, it is green to be prepared for water white transparency jaundice for fusing in air
Light glass.The jaundice green light glass luminous intensity of technique preparation is high, brightness is high, coloration is pure, glass melting temperature is low, glass forming ability is excellent
Good, preparation process is simple, thermal stability and chemical stabilization are excellent.It is produced according to the jaundice green light glass that preparation method of the present invention obtains
Product colour stable, colour rendering index are high, and color reducibility is good；In addition, the jaundice green light glass obtained according to preparation method of the present invention
The product transparency is good, and it is easy to prepare, simple for process, suitable for industrialized production.Prepared water white transparency jaundice green light glass can
For white light emitting device, also effective excitation available for blue light-emitting diode (LED).Therefore, it is prepared with this method
Mixing yttrium jaundice green light glass has considerable economic and social benefit, and application prospect is very wide.
Claims (4)
1. a kind of preparation method for mixing yttrium jaundice green light glass, it is characterised in that include the following steps：
1) first, by molar fraction by the Tb of 18~22mol%2O3, the B of 22~26mol%2O3, the Ga of 11~15mol%2O3,
The Y of 2~6mol%2O3, the GeO of 13~17mol%2, the SiO of 20~24mol%2, the Sb of 0~1mol%2O3, 0.3~
The SnO of 1mol%2, the ZrO of 0.3~1mol%2It mixes to being formed uniformly batch；
2) secondly, batch addition has been warming up in 1450~1500 DEG C of platinum crucible, has kept the temperature 30 minutes；
3) furnace temperature then, is cooled to 1380 DEG C by 30 minutes, and keeps the temperature 30min；
4) finally, the glass metal of melting is poured into 250~380 DEG C of graphite jig, is put into after sizing in 710 DEG C of stove, protected
After warm 3h, room temperature is cooled to 1 DEG C/min of rate of temperature fall and mixes yttrium jaundice green light glass up to transparent.
2. the preparation method according to claim 1 for mixing yttrium jaundice green light glass, it is characterised in that：The B2O3By dividing
It analyses pure boric anhydride to introduce, GeO2It is introduced by analytically pure germanium dioxide, Tb2O3、Ga2O3、Y2O3、Sb2O3, SnO2, ZrO2Respectively by
Analytically pure terbium peroxide, gallium oxide, yttrium oxide, antimony oxide, tin oxide, zirconium oxide introduce.
3. the preparation method according to claim 1 for mixing yttrium jaundice green light glass, it is characterised in that：The SiO2Using
The quartz sand of 60 mesh, wherein, the content of di-iron trioxide is less than 100ppm in quartz sand.
4. the preparation method according to claim 1 for mixing yttrium jaundice green light glass, it is characterised in that：The step 1)
It mixes to the uniformity to be more than after 98% and forms batch.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711432649.0A CN108164132B (en) | 2017-12-26 | 2017-12-26 | Preparation method of yttrium-doped yellow green light-emitting glass |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711432649.0A CN108164132B (en) | 2017-12-26 | 2017-12-26 | Preparation method of yttrium-doped yellow green light-emitting glass |
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| CN108164132A true CN108164132A (en) | 2018-06-15 |
| CN108164132B CN108164132B (en) | 2020-11-06 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1207086A (en) * | 1996-09-04 | 1999-02-03 | 保谷株式会社 | Glass for information recording medium substrate and glass substrate |
| CN101209894A (en) * | 2007-12-21 | 2008-07-02 | 华东师范大学 | Inorganic borosilicate luminescent glass and preparation thereof |
| CN102596840A (en) * | 2009-08-10 | 2012-07-18 | 海洋王照明科技股份有限公司 | Green light emitting glass used for ultraviolet LED and preparation method thereof |
| CN103288346A (en) * | 2013-04-27 | 2013-09-11 | 厦门百嘉祥微晶材料科技股份有限公司 | Microcrystalline glass substrate formula of light emitting diode, and preparation method |
| US8679587B2 (en) * | 2005-11-29 | 2014-03-25 | State of Oregon acting by and through the State Board of Higher Education action on Behalf of Oregon State University | Solution deposition of inorganic materials and electronic devices made comprising the inorganic materials |
| CN104039725A (en) * | 2012-01-12 | 2014-09-10 | 肖特公开股份有限公司 | Highly transmissive glasses with high solarisation resistance, use thereof and method for production thereof |
-
2017
- 2017-12-26 CN CN201711432649.0A patent/CN108164132B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1207086A (en) * | 1996-09-04 | 1999-02-03 | 保谷株式会社 | Glass for information recording medium substrate and glass substrate |
| US8679587B2 (en) * | 2005-11-29 | 2014-03-25 | State of Oregon acting by and through the State Board of Higher Education action on Behalf of Oregon State University | Solution deposition of inorganic materials and electronic devices made comprising the inorganic materials |
| CN101209894A (en) * | 2007-12-21 | 2008-07-02 | 华东师范大学 | Inorganic borosilicate luminescent glass and preparation thereof |
| CN102596840A (en) * | 2009-08-10 | 2012-07-18 | 海洋王照明科技股份有限公司 | Green light emitting glass used for ultraviolet LED and preparation method thereof |
| CN104039725A (en) * | 2012-01-12 | 2014-09-10 | 肖特公开股份有限公司 | Highly transmissive glasses with high solarisation resistance, use thereof and method for production thereof |
| CN103288346A (en) * | 2013-04-27 | 2013-09-11 | 厦门百嘉祥微晶材料科技股份有限公司 | Microcrystalline glass substrate formula of light emitting diode, and preparation method |
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